Water → 3,4-dihydro-2H-thieno[3,2-b]indole
반응식
[C:1]1([NH:7]N)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[S:9]1[CH2:13][CH2:12][C:11](=O)[CH2:10]1.O>C(O)(=O)C>[S:9]1[C:10]2[C:2]3[CH:3]=[CH:4][CH:5]=[CH:6][C:1]=3[NH:7][C:11]=2[CH2:12][CH2:13]1참가 물질
5
반응 조건
- 온도
- 80 °C
실험 절차
To a solution of phenylhydrazine (5.0 g, 46 mmole) in acetic acid (50 ml) was added dihydro-thiophen-3-one (4.72 g, 46 mmole) at room temperature. Following an exothermic reaction, the temperature was maintained at 80° C. for 2 h. The reaction mixture was poured into water (300 ml) and the precipitate was filtered. Purification on a short column of aluminum oxide (activity II, 6% water) using t-butylmethylether as the eluting solvent gave pure 3,4-dihydro-2H-thieno[3,2-b]indole as a yellow solid (3.9 g, 48% yield), m.p. 152-155° C. (lit. m.p. 153° C., WO01/12603) Step 2
후처리
- customan exothermic reaction
- filtrationthe precipitate was filtered
- customPurification on a short column of aluminum oxide (activity II, 6% water)
출처 및 근거
- ORD 기록
- ord-b57c3233657843b996544f76991d9455
- 출처 데이터셋
- uspto-grants-2005_02
- 특허 번호
- US06852726B2
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